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#$Date: 2016-03-23 15:48:26 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179348 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/45/4324587.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4324587
loop_
_publ_author_name
'Paul J. Calderone'
'Paul M. Forster'
'Lauren A. Borkowski'
'Simon J. Teat'
'Mikhail Feygenson'
'Meigan C. Aronson'
'John B. Parise'
_publ_contact_author_address
;Department of Geosciences
255 Earth and Space Sciences Building 
Stony Brook University
Stony Brook, NY 11794-2100
;
_publ_contact_author_email       jparise@notes.cc.sunysb.edu
_publ_contact_author_fax         '1-631-632-8240 '
_publ_contact_author_name        'John B. Parise'
_publ_contact_author_phone       '1-631-632-8196 '
_publ_section_title
;
 Ionothermal Synthesis and Magnetic Studies of Novel Two-Dimensional
 Metal-Formate Frameworks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2159
_journal_page_last               2167
_journal_paper_doi               10.1021/ic1015548
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C3 H5 Co O7, C3 H10 O N'
_chemical_formula_sum            'C6 H15 Co N O8'
_chemical_formula_weight         288.12
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.1298(8)
_cell_length_b                   16.1312(15)
_cell_length_c                   16.7808(16)
_cell_measurement_reflns_used    9228
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.55
_cell_measurement_theta_min      3.82
_cell_volume                     2200.7(4)
_computing_cell_refinement       'Bruker SAINT v7.56a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v7.56a'
_computing_molecular_graphics    'ORTEP-3 V 2.02'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22097
_diffrn_reflns_theta_full        33.62
_diffrn_reflns_theta_max         33.62
_diffrn_reflns_theta_min         3.33
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.000
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.5879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 Bruker AXS Madison WI USA'
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_description       plates
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.632
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3341
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.636
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0717P)²+3.2233P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                3003
_reflns_number_total             3341
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1015548_si_002_4.cif
_cod_data_source_block           structure4
_cod_database_code               4324587
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 0.76237(2) 0.192145(10) 0.620618(10) 0.01134(7) Uani 1 1 d .
O7 O 1.16932(11) 0.15107(6) 0.76853(5) 0.01702(18) Uani 1 1 d .
O1 O 0.77357(12) 0.31428(6) 0.66820(6) 0.01631(18) Uani 1 1 d D
HWA1 H 0.754(2) 0.3520(12) 0.6358(12) 0.024 Uiso 1 1 d D
HWA2 H 0.708(2) 0.3224(12) 0.7027(11) 0.024 Uiso 1 1 d D
O6 O 1.02319(11) 0.28594(6) 0.42169(5) 0.01649(17) Uani 1 1 d .
O4 O 0.99711(11) 0.16291(6) 0.66625(5) 0.01585(17) Uani 1 1 d .
O5 O 0.78142(15) -0.05997(6) 0.57149(6) 0.0228(2) Uani 1 1 d .
C5A C 1.27427(17) 0.44432(8) 0.63128(9) 0.0191(3) Uani 1 1 d .
H6A H 1.3468 0.4422 0.5839 0.023 Uiso 1 1 calc R
H7A H 1.3433 0.4564 0.6785 0.023 Uiso 1 1 calc R
O8A O 1.08597(12) 0.36405(6) 0.71147(6) 0.02055(19) Uani 1 1 d D
H10A H 0.996(2) 0.3466(12) 0.6999(13) 0.031 Uiso 1 1 d D
O3 O 0.85030(11) 0.24885(6) 0.51728(5) 0.01766(18) Uani 1 1 d .
N1A N 1.22225(14) 0.58951(7) 0.58808(7) 0.0178(2) Uani 1 1 d D
C1 C 0.78245(16) 0.01079(8) 0.60309(8) 0.0183(2) Uani 1 1 d D
H12 H 0.798(2) 0.0129(11) 0.6556(9) 0.022 Uiso 1 1 d D
C4A C 1.14733(17) 0.51260(9) 0.62069(8) 0.0205(2) Uani 1 1 d .
H4A H 1.0599 0.4932 0.5841 0.025 Uiso 1 1 calc R
H5A H 1.0958 0.5250 0.6728 0.025 Uiso 1 1 calc R
O2 O 0.75802(12) 0.07743(6) 0.56730(6) 0.01968(19) Uani 1 1 d .
C2 C 0.98204(15) 0.24125(8) 0.48043(7) 0.0159(2) Uani 1 1 d D
H11 H 1.048(2) 0.2013(9) 0.4954(11) 0.019 Uiso 1 1 d D
C3 C 1.03653(15) 0.17465(7) 0.73828(7) 0.0143(2) Uani 1 1 d D
H13 H 0.968(2) 0.2012(10) 0.7697(10) 0.017 Uiso 1 1 d D
C6A C 1.18961(19) 0.36158(8) 0.64208(8) 0.0224(3) Uani 1 1 d .
H8A H 1.1225 0.3489 0.5944 0.027 Uiso 1 1 calc R
H9A H 1.2730 0.3173 0.6482 0.027 Uiso 1 1 calc R
H1A H 1.310(2) 0.6062(14) 0.6171(11) 0.034 Uiso 1 1 d D
H2A H 1.148(2) 0.6305(11) 0.5870(13) 0.034 Uiso 1 1 d D
H3A H 1.258(2) 0.5813(14) 0.5380(10) 0.034 Uiso 1 1 d D
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Co Co 0.1760 1.1404
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Co1 O3 92.22(4) . .
O2 Co1 O6 89.34(4) . 4_456
O3 Co1 O6 87.85(4) . 4_456
O2 Co1 O4 88.41(4) . .
O3 Co1 O4 95.15(4) . .
O6 Co1 O4 176.32(4) 4_456 .
O2 Co1 O7 95.43(4) . 6_557
O3 Co1 O7 172.26(4) . 6_557
O6 Co1 O7 91.08(4) 4_456 6_557
O4 Co1 O7 86.23(4) . 6_557
O2 Co1 O1 175.98(4) . .
O3 Co1 O1 83.76(4) . .
O6 Co1 O1 90.61(4) 4_456 .
O4 Co1 O1 91.84(4) . .
O7 Co1 O1 88.59(4) 6_557 .
C3 O7 Co1 124.74(8) . 6_657
Co1 O1 HWA1 115.1(15) . .
Co1 O1 HWA2 113.2(14) . .
HWA1 O1 HWA2 103(2) . .
C2 O6 Co1 127.13(8) . 4_556
C3 O4 Co1 122.86(8) . .
C6A C5A C4A 110.15(12) . .
C6A C5A H6A 109.6 . .
C4A C5A H6A 109.6 . .
C6A C5A H7A 109.6 . .
C4A C5A H7A 109.6 . .
H6A C5A H7A 108.1 . .
C6A O8A H10A 109.2(15) . .
C2 O3 Co1 131.72(8) . .
C4A N1A H1A 111.9(14) . .
C4A N1A H2A 110.2(14) . .
H1A N1A H2A 109(2) . .
C4A N1A H3A 110.8(15) . .
H1A N1A H3A 107.0(19) . .
H2A N1A H3A 108.0(19) . .
O2 C1 O5 125.29(12) . .
O2 C1 H12 117.7(12) . .
O5 C1 H12 116.9(12) . .
N1A C4A C5A 111.70(11) . .
N1A C4A H4A 109.3 . .
C5A C4A H4A 109.3 . .
N1A C4A H5A 109.3 . .
C5A C4A H5A 109.3 . .
H4A C4A H5A 107.9 . .
C1 O2 Co1 124.30(9) . .
O3 C2 O6 123.98(11) . .
O3 C2 H11 117.4(12) . .
O6 C2 H11 118.6(12) . .
O7 C3 O4 124.09(11) . .
O7 C3 H13 117.0(12) . .
O4 C3 H13 118.9(12) . .
O8A C6A C5A 109.83(11) . .
O8A C6A H8A 109.7 . .
C5A C6A H8A 109.7 . .
O8A C6A H9A 109.7 . .
C5A C6A H9A 109.7 . .
H8A C6A H9A 108.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O2 2.0557(10) .
Co1 O3 2.0868(9) .
Co1 O6 2.1000(9) 4_456
Co1 O4 2.1097(9) .
Co1 O7 2.1146(9) 6_557
Co1 O1 2.1278(10) .
O7 C3 1.2521(15) .
O7 Co1 2.1146(9) 6_657
O1 HWA1 0.832(16) .
O1 HWA2 0.799(15) .
O6 C2 1.2661(14) .
O6 Co1 2.1000(9) 4_556
O4 C3 1.2647(14) .
O5 C1 1.2586(16) .
C5A C6A 1.5125(19) .
C5A C4A 1.5198(19) .
C5A H6A 0.9900 .
C5A H7A 0.9900 .
O8A C6A 1.4378(17) .
O8A H10A 0.811(15) .
O3 C2 1.2428(15) .
N1A C4A 1.4865(18) .
N1A H1A 0.905(16) .
N1A H2A 0.898(15) .
N1A H3A 0.899(16) .
C1 O2 1.2473(17) .
C1 H12 0.891(15) .
C4A H4A 0.9900 .
C4A H5A 0.9900 .
C2 H11 0.877(14) .
C3 H13 0.881(14) .
C6A H8A 0.9900 .
C6A H9A 0.9900 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 HWA1 O5 0.832(16) 1.806(16) 2.6359(14) 175(2) 8_765
O1 HWA2 O8A 0.799(15) 1.872(16) 2.6548(14) 166(2) 6_557
O8A H10A O1 0.811(15) 1.952(15) 2.7608(14) 175(2) .
N1A H1A O4 0.905(16) 1.993(16) 2.8858(14) 168(2) 8_865
N1A H1A O7 0.905(16) 2.647(19) 3.3064(15) 130.4(17) 8_865
N1A H2A O6 0.898(15) 1.940(15) 2.8364(15) 175(2) 5_766
N1A H2A O3 0.898(15) 2.62(2) 3.2051(15) 123.8(16) 5_766
N1A H3A O5 0.899(16) 1.879(17) 2.7621(16) 166.8(19) 4_556
